Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | 2-ethoxy-2-thioxoAcetamide | HCID 21613763 | — |
| Reactant | HCID 58046377 | HCID 58046377 | — |
| Product | HCID 58046439 | HCID 58046439 | — |
Reaction Steps
2,2-Dibromo-1-(imidazo[1,2-b]pyridazin-3-yl)ethanone (790 mg, 2.48 mmol) and ethyl thiooxamate (547 mg, 3.96 mmol) were dissolved in 1,4-dioxane (24.8 mL) and heated to 100° C. for 4 h. The solution was cooled to room temperature and water was added. The aqueous layer was extracted with ethyl acetate (×3). The organic layers were combined and dried with magnesium sulfate, filtered, and concentrated under reduced pressure to give the title compound as an orange solid. 1H NMR (500 MHz, CD3SOCD3) δ 8.79 (s, 1H); 8.77 (d, 1H); 8.33 (s, 1H); 8.30 (d, 1H); 7.39 (dd, 1H); 4.43 (q, 2H); 1.36 (t, 3H). LRMS (APCI) calc'd for (C12H10N4O2S) [M+H]+, 275.1. found 275.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08592425B2 |
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| Source dataset | uspto-grants-2013_11 |
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| ORD ID | ord-6ea8403193834512b3959aa50a7787c0 |
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| Source note | uspto-grants-2013_11 |
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